Distillation flask and mounting



3 Sheets-Sheet l June 30, 1959 A. G. NERHEIM I DISTILLATION FLASK ANDMOUNTING Filedmamh 21,Y 1957 9%' fwd@ June 30, 1959 A. G. NERHEIM2,892,759

DISTILLATIGN FLASK AND MOUNTING Filed March 2i, 1957 s sheets-sheet 2June 30, 1959 A. G. NERHEIM 2,892,759

` DISTILLATION FLASK AND MOUNTING Filed March 21, 1957V v5 Sheets-Sheet5 lama Mmeg

DISTILLATION FLASK AND MOUNTING Arvie Glenn'Nerhem, Calumet City, Ill.,assignor to Standard Oil Company, Chicago, Ill., a corporation ofIndiana Application March 21, 1957, Serial No. 647,662

3 Claims. (Cl. 202-235) This invention relates to improved fractionatorcolumns of the type known as lspinning band columns. More particularly,the invention relates to distilling flask constructions for such afractionator.

In a spinning band column, the complete unit comprises in general astill pot for holding the charge, a fractionating column or tube, acondenser system, a liquid product receiver, and a rotatable elementdisposed within the fractionating column. Conventionally, spinning bandcolumns of the type to which my improvements relate employ a rotatableelement comprising a metallic band having a cross-sectional area whichis substantially less than the flow area of the column. Controllableheating means are provided for supplying heat to the still pot, thestill pot and heating element ordinarily being enclosed withina vacuumliask which is removably seated at its upper end in contact with avacuum jacket which substantially encloses the fractionatng column andtake-off line. Throughput in a spinning band column is conventionallycontrolled by controlling the heaters; however, it has been found thatcolumn eiiiciency may be increased by increasing the rotation speed ofthe spinning band. However, if vibration occurs in spinning band columnsand if frictional heat of Yrotation is generated, the eiiiciency islower.

4Distilling flask assemblies heretofore used are not easily rechargedand further misalignment of the distilling flask assembly may break thecolumn-flask joint. Bumping the flask out of alignment or attempting toremove a flask frozen to the column also have resulted in breaking thecolumn-flask joint.

' It is therefore, an object of my invention to provide a distillingflask assembly which avoids these difliculties. Thus, it is a furtherobject of the invention to provide a distilling flask assembly whichwill permit recharging of the sample, which gives protection to thecolumn, which is less expensive and ofsimpler construction thanheretofore used, and which may be adapted for use on conventionalfractionating columns. The above and other objects of the invention willbecome apparent as the detailed description thereof proceeds. Y

Further details and advantages of my invention will become apparent asthe description thereof proceeds with reference to the accompanyingdrawings wherein:

Figure 1 is a vertical section showing the spinning band drive, headconstruction and distillation iiask;

Figure 2 is a top view, partly in section, of the head viewed along theline 2 2 with parts removed in Figure 1;

Figure 3 is an elevation, partly in section, of the adjustable asksupport;

Figure 4 is a side view of the apparatus in Figure 3;

Figure 5 is a section taken along line 5--5 in Figure 3;

Figure 6 is a fragmentary side elevation taken along the line 6-6 inFigure 3; and

Figure 7 is a fragmentary plan view, taken along the line 7-7 in Figure3.

Referring to Figures l and 2 of the drawings, a column ate t 10comprising a relatively long thin glass tube, contains the spinning bandllhaving a drive shaft 12 which extends through the head 13 and issecured to the drive pin 14 within the magnetic coupling 15. Thiscoupling 15 includes a pair of opposed magnets 16 and 17 arrangedaxially of each other and of the shaft 12. The drive magnet 16 issecured, for example, by a chuck means 13 so that it may be driven, andthe other magnet 17 is within a vacuum-tight and non-magnetic housing 19which is fixed to the head 13 by means of a standard tapered joint 20engaging a corresponding tapered joint 21 in head 13.

The elongated drive pin 14 disposed within the separable housing 19 isarranged to be rotated with the enclosed magnet 17. An antifrictionbearing means 22 rotatably supports the drive pin 14 within the housing19. The drive shaft 12, xed to drive pin 14, extends longitudinally fromthe lower end of the housing 19, through the head 13, and engages tfheband shaft 23 which in turn supports the rotatable element on band 11.

The rotatable band 11 is slightly smaller in its greatest lateraldimension than the internal diameter of the fractionating tube or column10. Rotation of the close-itting band 11 produces a wetted wall effectwithin the fractionating tube 10 with the result that there is intimatecontact between the up-flowing vapors within the column 10 and thedown-ilowing reflux on the wall thereof.

The head 13 includes a tapered body 24 arranged in a vacuum-tight sealwith the seat 2S at the upper end of the column 10. The head 13 includeslaterally-extending condenser inlet 26 and outlet 27, each passingthrough the side wall thereof and being connected to opposite ends ofthe looped condenser 28 which depends below the hollow body 24 into thetop of the column 10. A drip tip 29 is provided on each of the separatelegs of the condenser 28. A vacuum connection 30, also laterallyextending from the side wall of head 13, permits vacuum operation of thecolumn 10' and completes the construction of head 13.

The leads 31 to thermocouple 32 pass through the housing 19 and thetherrnocouple 32 is disposed adjacent the upper end of the spinning band11 and soldered in place. The solenoid 33 is aligned with the soft ironcore 34 embedded within a cavity 35 in housing 19. Immediately below theexposed inner end of the core 34 is arranged the upper paramagnetic end36 of the needle shaft 37 which passes within the needle guide bore 39in housing 19 and the needle tip 40 is on the needle seat 41. The needletip 40 is thus raised from the seat 41 by the action of theelectromagnet bar or core 34 on the paramagnetic top 36 of the needle 37when the solenoid coil 33 -is energized.

A condenserv 28 comprises a loop of tubing which doubles back on itselfwith a pair of drip tips 29 at the lower extremities of the loop whichdischarges on the edge of the needle seat 41. When the needle tip 40 israised from the seat 41, the condensate is removed from the column bytake-oid:` line 42 into a receiver (not shown). By regulating the ow ofcooling fluid into the total condenser 28, the evolved vapors within thefractionating tube 10 may be condensed and returned as reiiux when thetake-olf line 42 is closed by the needle valve.

Condensate is prevented from leaking past the needle seat 41 byalignment of the needle 37 and by keeping the tip 46 clean. The head 13should be adjusted rso that the needle 37 is vertical and moves freelywithin the guide bore 39. It will be understood that the paramagneticend 36 of the needle 37 is disposed immediately below the inner end ofthe bar 34 and is lifted thereby when the coil 33 is energized.

Referring to Figures 3 to 7 showing the distillation flask and mounting,I provide a flask 50 which is simply set on a heater 51. An insulatingdewar flask 52 contains the distilling fiask 50, and a glass wool collar53 closes the flask 52. The distillation flask 50 is provided with athermocouple well 54 and the thermocouple leads 55 extend over the topof the dewar ask 52. The heater 51 is supported by a coil spring 56disposed within the dewar flask 52. The heater leads 57 pass through theglass wool collar 53 and from the dewar flask 52.

The flask 50 is pear-shaped and set in a cone-shaped heater 51 mountedon a spring 56. The entire apparatus is insulated with a dewar ask S2and a glass wool collar 53. A support device 58 yfor the flask 52 issecured to the dewar flask 52 permitting it to be swung directly underthe column and up into the aligning guide 59 which positions the flaskfor charging. The contents of the ask l5i) are stirred with a wireimpellor V68 fixed to the .lower end of the spinning band 11.

The aligned distilling ilask 50 is fixed to the lower end of the column10. The dewar flask 52 is lifted by raising the mounting 58 on the'slide rods 61 and .disposed about the distilling flask 50 therebyproviding effective insulation throughout the distillation.

The particular elements of the apparatus covered by Figures 3 to 8 arethe slide rods 61 with aligning guide 59, flask 'support device 58, theheater 51 and flask 50. The tops of the two slide rods 61 are securedwith connectors 68 welded to the edges of a clamp 69 which is bolted tothe column support 70 just above the ask joint 71. The bottom of sliderods 61 are set in the foot 72 welded to a base 73 below the column 10.The aligning guide 59, comprising a metal strip welded to a connector68, is fastened to the right slide rod 61.

The flask support device 58 pivots around the left slide rod 61 on aleveling apparatus 74 (Figures 3 and 5) that pinches the rod 61 to holdthe support 58 ata desired height above the base 73. The support 58clamps around a pint dewar flask 52 with support lip 76 sliding up underthe aligning guide 59 to steer the support 58 as it is raised to thedesired position below the column 10.

The heater 51 is a metal cone Wound with high resistance wire andinsulated. Two clamps 77 protect this wiring and hold the supportingcoil spring 56 in place. .A variety of flask sizes ranging from 25-200ml. may be used. If the ask freezes to the column, it can be removedeasily by simply heating the ask .joint with a torch.

When the distillation is complete, the dewar ask 52 can be lowered onsupport 58 and this quickly cools the distilling flask 50 which permitsits prompt removal from the column .10. These features permit moreeflicient distillation in less time and at less cost than distillationilask assemblies heretofore used with spinning band columns.

The appartus has been described as including an eX- terior permanentmagnet. An electromagnet may be substituted on the housing, enclosingthe interior permanent magnet, surrounded by field windings so that theenclosed magnet comprises a rotor or amature of a motor.

This application is a continuation-impart of my now abandonedapplication Serial No. 596,584, filed July 9, 1956, and entitledSpinning Band Fractionator.

Although the invention has been described with reference to a preferredembodiment thereof, it is to be understood that this is by way ofillustration only. Accordingly, it is contemplated that modificationsand variations can be made in the apparatus by those skilled Ain theartin light of the preceding description and without departing from thespirit ofthe invention.

What I claim is:

1. An improved distillation flask assembly which comprises incombination a pear-shaped distillation flask, a standard tapered jointin the upper end of said distillation flask, a well in the lower end ofsaid flask, a cone heater for said ask disposed about the lower endthereof and encircling said well, an open-topped insulating housingaccommodating said heater and said flask, coil spring support meansbetween the bottom end of said housing and said heater, a removableinsulating collar enclosing the top of said housing and encircling theupper end of said flask, an adjustable support for said housing, saidadjustable support including a base, a pair of upstanding rods on saidbase, a swingable clamping arm hingedly xed to one of said rods,vertical guide means carried by the second of said rods, a projection ofsaid clamping arm adapted to move within said guide, said guide meanscomprising an open-ended slot terminating above said base and open atits lower end to pass said projection, and means associated with saidVhingedly fixed arm for vertically adjusting said support.

2. An improved distillation flask support assembly including a base, apair of spaced upstanding rods on said base, a horizontally swingableclamping arm hingedly fixed to one of said rods, vertical guide meanscarried by the second of said rods and terminating a substantialdistance above said base, a projection in said clamping arm adapted tomove vertically within and below `said guide means, and means associatedwith said hingedly fixed clamping arm for vertically adjusting saidsupport assembly downwardly below said guide means to permit horizontalrotation of said arm.

3. A distillation flask assembly and retractable -support Vthereforwhich comprises a distillation ask having a constricted bottom portion,a cone heater for said flask disposed about and below said bottomportion, an insulated housing containing said heater and said flask, aretractable support for said housing, said support including ahorizontal swingable clamping arm, arrst upright slide rod, verticallyadjustable friction holder means securing Asaid arm to said slide rod, asecond slide rod parallel to said first slide rod, an aligning guidemember supported by said second slide rod, said guide member beingsubstantially shorter than said slide rod and secured thereto only atits upper end, a guide tongue carried by the outer end of said arm,Vsaid tongue and said aligning guide member cooperating to normallyrestrain said arm against horizontal rotation, whereby lowering said armby adjustment of said friction holder means retractssaid tongue fromwithin said guide member thereby permitting the horizontal nrotation ofsaid arm and said insulated housing containing lsaid ask and heater.

Laboratory for the Synthetic Liquid Fuels Program, (Feldman,Pantazoplos, and Orchin), Bureau of Mines, Report of Investigations 4764(Fig. 2 relied on).

1. AN IMPROVED DISTILLATION FLASK ASSEMBLY WHICH COMPRISES INCOMBINATION A PEAR-SHAPED DISTILLATION FLASK, A STANDARD TAPERED JOINTIN THE UPPER END OF SAID DISTILLATION, A WELL IN THE LOWER END OF SAIDFLASK, A CONE HEATER FOR SAID FLASK DISPOSED ABOUT THE LOWER END THEREOFAND ENCIRCLING SAID WELL, AN OPEN-TOPPED INSULATING HOUSINGACCOMMODATING SAID HEATER AND SAID FLASK, COIL SPRING SUPPORT MEANSBETWEEN THE BOTTOM END OF SAID HOUSING AND SAID HEATER, REMOVABLEINSULATING COLLAR ENCLOSING THE TOP OF SAID HOUSING AND ENCIRCLING THEUPPER END OF SAID FLASK, AN ADJUSTABLE SUPPORT FOR SAID HOUSING, SAIDADJUSTABLE SUPPORT INCLUDING A BASE A PAIR OF UPSTANDING RODS ON SAIDBASE, A SWINGABLE CLAMPING ARM HILNGEDLY FIXED TO ONE SAID RODS,VERTICAL GUIDE MEANS CARRIED BY THE SECOND OF SAID RODS, A PROJECTION OFSAID CLAMPING ARM ADAPTED TO MOVE WITHIN SAID GUIDE, SAID GUIDE MEANSCOMPRISING AN OPEN-ENDED SLOT TERMINATING ABOVE SAID BASE AND OPEN ATITS LOWER END TO PASS SAID PROJECTION, AND MENS ASSOCIATED WITH SAIDHINGEDLY FIXED ARM FOR VERTICALLY ADUSTING SAID SUPPORT.